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CN101049328A - Technique for producing extractive of olive growing leaves - Google Patents

Technique for producing extractive of olive growing leaves Download PDF

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Publication number
CN101049328A
CN101049328A CN 200710107642 CN200710107642A CN101049328A CN 101049328 A CN101049328 A CN 101049328A CN 200710107642 CN200710107642 CN 200710107642 CN 200710107642 A CN200710107642 A CN 200710107642A CN 101049328 A CN101049328 A CN 101049328A
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Prior art keywords
leaf
extract
olive
growing leaves
oleae europaeae
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CN 200710107642
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姚自奇
温凯
白小勇
付军
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TIANYUAN OIL OLIVE TECH DEVELOPMENT Co Ltd LONGMAN
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TIANYUAN OIL OLIVE TECH DEVELOPMENT Co Ltd LONGMAN
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Abstract

A process for preparing the extract of olive leaf includes such steps as low-temp drying in dark condition, pulverizing, extracting in ethanol or methanol by reflux, immersing, seeping, or ultrasonic wave, filtering, vacuum concentrating, vacuum drying to obtain coarse extract, pulverizing, sieving, dissolving in water, filtering, membrane separation, and purifying by ion exchange.

Description

Technique for producing extractive of olive growing leaves
Technical field
The present invention relates to a kind of production technology of olive leaf extract.
Background technology
Fructus oleae europaeae, (Olea europaea L.) claims olive, Europe Fructus Canarii albi, olive again, is Oleaceae (Oleaceae) Olea (Olea L) plant, is that famous and precious evergreen woody oleiferous plants in the world and fruit are used seeds.Fructus oleae europaeae originates in Asia Minor, mainly is distributed in littoral area, Mediterranean, is to concentrate the place of production with Spain, Italy, Portugal and Albania.1964, when the Premier Zhou Enlai visits Albania, recognize after the special efficacy and extensive use of olive oil that decision is introduced and promoted.Introduce a fine variety the Fructus oleae europaeae expert effort of decades through China, introduce a fine variety and obtained success.The Fructus oleae europaeae output of normal region has reached the level in original producton location.According to incompletely statistics, existing about 400,000 mu of the Fructus oleae europaeae area (1,000 ten thousand strain) of China.
Fructus oleae europaeae is the conventional medicament of Mediterranean Region, is used for the treatment of multiple disease with leaf and fruit medicine.The decoct of Folium olive or preserved material have certain curative effect in the medication among the people of mediterranean country Chang Zuowei diabetes.Olive leaf extract is used as dietary supplement with raise immunity in America and Europe.Modern data shows that Fructus oleae europaeae has anti-arrhythmia, antifungal, anti-hypercholesterolemia, blood sugar lowering, blood pressure lowering, antiinflammatory, antioxidation, antiviral, diuresis, the multiple pharmacologically active of central nervous system such as spasmolytic and vasodilation, be used for the treatment of diabetes, hypertension, diarrhoea, edema, the intestines and stomach angor, herpes, respiratory tract infection, constipation, diseases such as urinary tract infection.Separating the chemical constituent that obtains from leaf of Fructus oleae europaeae can be divided into: flavonoid, secoiridoid class, saccharide, organic acid and other chemical compound.Olive leaf extract has many middle functions such as blood sugar lowering, blood fat reducing, bacteriostatic activity, antioxidant activity, anti-inflammatory activity enhance immunity and beauty treatment, and potentiality to be exploited is huge.Modern biotechnology the analysis showed that active substance mainly contains olive polyphenol, flavonoid, secoiridoid class (comprising cleupin) etc. in the leaf of Fructus oleae europaeae, and its antioxidation biology active matter content is higher than Fructus oleae europaeae fruit and stem.
At present domestic have report to extract the processing Fructus Canrii Albi extract with Folium olive and leaf of Fructus oleae europaeae, but adopt mostly water carry or alcohol extraction after direct spray drying composition, cleupin, total phenols and flavones content are low in the product, are starkly lower than external required standard extractive content.The present invention's extraction, separation and purification to the Folium olive effective ingredient on traditional handicraft extraction, isolating basis improves, to improve separation and purification efficient.The present invention adopts reflux, extract,, percolation to extract and ultrasonic extracting method such as auxiliary, and membrane separation technique and ion exchange technique method that vacuum concentration, drying, crude extract take microfiltration, ultrafiltration, nanofiltration to combine are carried out purification; Contrast with traditional leach extraction method, determine best extraction, the scheme of separation and purification.The application of membrane separation technique in extracting effective ingredients in plant obtained very big development in recent years, is a kind of promising new technology.Ultrasonic assisted extraction method is ultrasound wave and conventional solvent extraction method to be combined and a kind of new extracting method that forms.Compare with conventional extraction method have applied widely, that raw material is handled is convenient, extraction efficiency is high, save time, save advantage such as solvent.
Summary of the invention
The object of the present invention is to provide a kind of production technology that yield height and extract active constituent content height and extract mainly contain the olive leaf extract of cleupin, total phenols and three kinds of compositions of flavone of extracting.
Purpose of the present invention realizes by following manner:
Figure A20071010764200041
1. with leaf of Fructus oleae europaeae low-temperature dark drying, pulverize;
2. the leaf of Fructus oleae europaeae after pulverizing adds 1~20 times of ethanol or methanol extraction;
3. leachate is filtered, vacuum concentration, vacuum drying gets the leaf of Fructus oleae europaeae crude extract;
4. crude extract is pulverized, crossed 20~80 mesh sieves, the after-filtration that is dissolved in water is removed impurity;
5. through membrance separation, the ion exchange separation and purification gets the leaf of Fructus oleae europaeae extract.
Technique for producing extractive of olive growing leaves of the present invention can add the leaf of Fructus oleae europaeae after pulverizing 1~20 times of ethanol or methanol eddy and extract.
Technique for producing extractive of olive growing leaves of the present invention also can add the leaf of Fructus oleae europaeae after pulverizing 1~20 times of ethanol or methanol dipping and extract determining alcohol 30~95%, 25~65 ℃ of extraction temperatures, extraction time 36~144h; Agitation as appropriate is to increase extraction efficiency in the leaching process.
Technique for producing extractive of olive growing leaves of the present invention also can add the leaf of Fructus oleae europaeae after pulverizing 1~20 times of ethanol or methanol percolation and extract.
Technique for producing extractive of olive growing leaves of the present invention also can add 1~20 times of ethanol or methanol ultrasonic extraction, frequency 20~80kHz, time 20~180min, 20~55 ℃ of temperature with the leaf of Fructus oleae europaeae after pulverizing.
The described vacuum concentration temperature of technique for producing extractive of olive growing leaves of the present invention is no more than 55 ℃.
The described vacuum drying temperature of technique for producing extractive of olive growing leaves of the present invention is no more than 55 ℃.
The employed film of technique for producing extractive of olive growing leaves of the present invention sees table 1 for details.The present invention utilizes membrane separation technique, with the diffusion barrier of PSPP, the leaf of Fructus oleae europaeae extracting solution is divided into different fraction by the size of molecular weight, to the part that cleupin content is concentrated carried out concentrating, dry, analyze.
The present invention compared with prior art, it is reasonable to have a process route, the extraction ratio height, good product quality is suitable for advantages such as suitability for industrialized production.Extract mainly contains cleupin, total phenols and three kinds of effective ingredient of flavone.The extraction ratio of its crude extract is 10~25%, and product cleupin content reaches 2~6%, and flavones content reaches 20~30%, and polyphenol content reaches 8~12%.The olive leaf extract technical specification sees Table 2.
The specific embodiment
The following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
Embodiment 1
Get the exsiccant leaf of Fructus oleae europaeae of 100kg, pulverize, add 10 times of 90% alcohol reflux, leachate is filtered, vacuum concentration, vacuum drying concentrates and baking temperature is no more than 55 ℃, gets leaf of Fructus oleae europaeae crude extract 16kg.Crude extract is pulverized, crossed 80 mesh sieves, the after-filtration that is dissolved in water, through membrance separation, the ion exchange separation and purification gets leaf of Fructus oleae europaeae extract 1.8kg.
Embodiment 2
Get the exsiccant leaf of Fructus oleae europaeae of 100kg, pulverizing adds 15 times of 80% methanol eddy and extracts, leachate is filtered, and vacuum concentration, vacuum drying concentrates and baking temperature is no more than 55 ℃, gets leaf of Fructus oleae europaeae crude extract 13kg.Crude extract is pulverized, crossed 60 mesh sieves, the after-filtration that is dissolved in water, through membrance separation, ion exchange separates alcoholization, gets leaf of Fructus oleae europaeae extract 1.5kg.
Embodiment 3
Get the exsiccant leaf of Fructus oleae europaeae of 100kg, pulverize, add 10 times of 85% alcohol dipping and extract 2 times, each 48h, 55 ℃ of extraction temperatures merge lixiviating solution, filter, vacuum concentration, vacuum drying concentrates and baking temperature is no more than 55 ℃, leaf of Fructus oleae europaeae crude extract 19kg.Crude extract is pulverized, crossed 80 mesh sieves, the after-filtration that is dissolved in water, through membrance separation, ion exchange separates alcoholization, gets leaf of Fructus oleae europaeae extract 1.8kg.
Embodiment 4
Get the exsiccant leaf of Fructus oleae europaeae of 100kg, pulverize, add 20 times of 90% ethanol percolate extraction, will carry thing liquid and filter, vacuum concentration, vacuum drying concentrates and baking temperature is no more than 55 ℃, gets leaf of Fructus oleae europaeae and slightly extracts 15kg.Crude extract is pulverized, crossed 80 mesh sieves, the after-filtration that is dissolved in water, through membrance separation, ion exchange separates alcoholization, gets leaf of Fructus oleae europaeae extract 1.7kg.
Embodiment 5
Get the exsiccant leaf of Fructus oleae europaeae of 100kg, pulverize, add 20 times of 95% ethanol ultrasonic extraction, supersonic frequency 20kHz, each ultrasonic 2min, work is 0.2s intermittently, omnidistance time 45min, 45 ℃ of temperature repeat to extract twice, amount to 90min, thing liquid be will carry and vacuum concentration, vacuum drying filtered, concentrate with baking temperature and be no more than 55 ℃, get leaf of Fructus oleae europaeae and slightly extract 25kg.Crude extract is pulverized, crossed 80 mesh sieves, the after-filtration that is dissolved in water, through membrance separation, ion exchange separates alcoholization, gets leaf of Fructus oleae europaeae extract 2.4kg.
Embodiment 6
Get the exsiccant leaf of Fructus oleae europaeae of 100kg, pulverize, add 20 times of 80% methanol ultrasonic extraction, supersonic frequency 40kHz, each ultrasonic 2min, work is 0.2s intermittently, omnidistance time 50min, 45 ℃ of temperature repeat to extract twice, amount to 100min, thing liquid be will carry and vacuum concentration, vacuum drying filtered, concentrate with baking temperature and be no more than 55 ℃, get leaf of Fructus oleae europaeae and slightly extract 22kg.Crude extract is pulverized, crossed 80 mesh sieves, the after-filtration that is dissolved in water, through membrance separation, ion exchange separates alcoholization, gets leaf of Fructus oleae europaeae extract 2.1kg.
This institute of table 1. uses the key property and the manufacturer of film
Kind Molecular cut off Applicable pH Applicable temperature Manufacturer
Polysulfone membrane (PS) polypropylene screen (PAN) polysulfonamides film (PSA) composite 2000、4000 10000 70000,140000 500,1000 2~12 2~12 2~12 1~13 <50℃ <50℃ <50℃ 5~60℃ The Shanghai atomic nucleus is matched general film scientific ﹠ technical corporation
Table 2. olive leaf extract technical specification
Project Technical specification
Abnormal smells from the patient Bitter taste
Color and luster Bottle green is to brown
Character Powdery or paste
Moisture content ≤5%
Ash ≤5%
Heavy metal ≤10mg/kg
Granularity 80 orders
Total number of bacteria ≤1000cfu/g
Cleupin ≥2%
Total flavones ≥20%
Polyphenol ≥8%

Claims (10)

1. technique for producing extractive of olive growing leaves mainly may further comprise the steps:
1. with leaf of Fructus oleae europaeae low-temperature dark drying, pulverize;
2. the leaf of Fructus oleae europaeae after pulverizing is with ethanol or methanol extraction;
3. leachate is filtered, vacuum concentration, vacuum drying gets the leaf of Fructus oleae europaeae crude extract;
4. crude extract is pulverized, sieved, the after-filtration that is dissolved in water is removed impurity;
5. through membrance separation, the ion exchange separation and purification gets the leaf of Fructus oleae europaeae extract;
Olive leaf extract mainly contains cleupin, total phenols and three kinds of effective ingredient of flavone.
2. according to the described technique for producing extractive of olive growing leaves of claim 1, it is characterized in that 2. described ethanol of step or methanol concentration 30~95%.
3. according to the described technique for producing extractive of olive growing leaves of claim 1, it is characterized in that the 2. described pure extracting method of step is a reflux, extract.
4. according to the described technique for producing extractive of olive growing leaves of claim 1, it is characterized in that the 2. described pure extracting method of step extracts 1~20 times of pure consumption, determining alcohol 30~95%, 25~65 ℃ of extraction temperatures, extraction time 36~144h for dipping.
5. according to the described technique for producing extractive of olive growing leaves of claim 1, it is characterized in that the 2. described pure extracting method of step is that percolation extracts.
6. according to the described technique for producing extractive of olive growing leaves of claim 1, it is characterized in that the 2. described pure extracting method of step is a ultrasonic extraction, frequency 20~80kHz, time 20~180min, 20~55 ℃ of temperature.
7. according to the described technique for producing extractive of olive growing leaves of claim 1, it is characterized in that described vacuum concentration temperature is no more than 55 ℃; Described vacuum drying temperature is no more than 55 ℃.
8. according to the described technique for producing extractive of olive growing leaves of claim 1, it is characterized in that the 5. used film of step is polysulfone membrane (PS), polypropylene screen (PAN), polysulfonamides film (PSA) or composite.
9. according to the described technique for producing extractive of olive growing leaves of claim 1, it is characterized in that described olive leaf extract cleupin content 2~6%, flavones content 20~30%, polyphenol content 8~12%.
10. according to the described technique for producing extractive of olive growing leaves of claim 1, it is characterized in that described leaf of Fructus oleae europaeae is all leaf of Fructus oleae europaeae of Olea europaea kind (Olea europaea L) of Oleaceae (Oleaceae) Olea (Olea L).
CN 200710107642 2007-05-23 2007-05-23 Technique for producing extractive of olive growing leaves Pending CN101049328A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101912109A (en) * 2010-07-09 2010-12-15 中国林业科学研究院林产化学工业研究所 A kind of health food with anti-hypoxia function and preparation method thereof
CN102224958A (en) * 2011-05-18 2011-10-26 福州市鼓楼区大特生物技术有限公司 Method for extracting green olive juice with ultrasonic at low temperature
CN102260588A (en) * 2011-06-21 2011-11-30 西北师范大学 Method for synchronously extracting pomace oil and polyphenol from olive processing waste residue
CN101781344B (en) * 2009-12-13 2012-06-27 成都普思生物科技有限公司 Method for preparing olive leaf extract
CN102727409A (en) * 2012-07-04 2012-10-17 广东雅威生物科技有限公司 Moisturizing cream containing natural olive oil and derivatives of natural olive oil, and preparation method of moisturizing cream
CN103830332A (en) * 2012-11-20 2014-06-04 中国科学院兰州化学物理研究所 Method for extracting anti-diabetic active parts in olive leaf
CN104311613A (en) * 2014-09-30 2015-01-28 桂林三宝药业有限公司 Method for extracting oleuropein from olive leaves
CN104622971A (en) * 2013-11-07 2015-05-20 中国科学院兰州化学物理研究所 Pharmaceutical composition for resisting diabetes activity and preparation method thereof
CN107969552A (en) * 2017-12-24 2018-05-01 中国林业科学研究院林产化学工业研究所 A kind of extractive of olive growing leaves feed addictive and its application
CN110215423A (en) * 2019-06-19 2019-09-10 珠海远大美业生物科技有限公司 The anti-ageing composition of reparation containing various plants extract, preparation method and application
CN114468095A (en) * 2022-02-23 2022-05-13 兰州海关技术中心 Plant active tea and preparation method thereof
CN115444791A (en) * 2022-08-08 2022-12-09 何直源 Olive leaf fermented extract and its preparation method and application

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101781344B (en) * 2009-12-13 2012-06-27 成都普思生物科技有限公司 Method for preparing olive leaf extract
CN101912109A (en) * 2010-07-09 2010-12-15 中国林业科学研究院林产化学工业研究所 A kind of health food with anti-hypoxia function and preparation method thereof
CN101912109B (en) * 2010-07-09 2012-12-19 中国林业科学研究院林产化学工业研究所 Health-care food with hypoxia tolerance function and preparation method thereof
CN102224958B (en) * 2011-05-18 2013-05-22 福州市鼓楼区大特生物技术有限公司 Method for extracting green olive juice with ultrasonic at low temperature
CN102224958A (en) * 2011-05-18 2011-10-26 福州市鼓楼区大特生物技术有限公司 Method for extracting green olive juice with ultrasonic at low temperature
CN102260588A (en) * 2011-06-21 2011-11-30 西北师范大学 Method for synchronously extracting pomace oil and polyphenol from olive processing waste residue
CN102260588B (en) * 2011-06-21 2013-01-02 西北师范大学 Method for synchronously extracting pomace oil and polyphenol from olive processing waste residue
CN102727409B (en) * 2012-07-04 2013-05-29 广东雅威生物科技有限公司 Moisturizing cream containing natural olive oil and derivatives of natural olive oil, and preparation method of moisturizing cream
CN102727409A (en) * 2012-07-04 2012-10-17 广东雅威生物科技有限公司 Moisturizing cream containing natural olive oil and derivatives of natural olive oil, and preparation method of moisturizing cream
CN103830332A (en) * 2012-11-20 2014-06-04 中国科学院兰州化学物理研究所 Method for extracting anti-diabetic active parts in olive leaf
CN104622971A (en) * 2013-11-07 2015-05-20 中国科学院兰州化学物理研究所 Pharmaceutical composition for resisting diabetes activity and preparation method thereof
CN104311613A (en) * 2014-09-30 2015-01-28 桂林三宝药业有限公司 Method for extracting oleuropein from olive leaves
CN107969552A (en) * 2017-12-24 2018-05-01 中国林业科学研究院林产化学工业研究所 A kind of extractive of olive growing leaves feed addictive and its application
CN110215423A (en) * 2019-06-19 2019-09-10 珠海远大美业生物科技有限公司 The anti-ageing composition of reparation containing various plants extract, preparation method and application
CN114468095A (en) * 2022-02-23 2022-05-13 兰州海关技术中心 Plant active tea and preparation method thereof
CN115444791A (en) * 2022-08-08 2022-12-09 何直源 Olive leaf fermented extract and its preparation method and application

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